CN112979188B - Method for preparing volcanic ash active material from building residue soil - Google Patents
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- CN112979188B CN112979188B CN201911290595.8A CN201911290595A CN112979188B CN 112979188 B CN112979188 B CN 112979188B CN 201911290595 A CN201911290595 A CN 201911290595A CN 112979188 B CN112979188 B CN 112979188B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/24—Cements from oil shales, residues or waste other than slag
- C04B7/246—Cements from oil shales, residues or waste other than slag from waste building materials, e.g. waste asbestos-cement products, demolition waste
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/36—Manufacture of hydraulic cements in general
- C04B7/43—Heat treatment, e.g. precalcining, burning, melting; Cooling
- C04B7/44—Burning; Melting
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
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Abstract
The invention provides a method for preparing a volcanic ash active material from building residue soil, the main components of the building residue soil are clay substances with the granularity of less than 100 mu m, and the main mineral phases are quartz, mica and chlorite, and the method comprises the following steps: drying the building residue soil to remove moisture; then adding an activating auxiliary agent into the construction residue soil, calcining, and cooling to room temperature; ball milling to obtain the volcanic ash active material. The main minerals in the activated building residue soil are converted into amorphous state, the activated building residue soil has good hydrolytic capacity and reaction capacity, and the data shows that the activated building residue soil has pozzolanic activity, and the 28-day compressive strength can reach about 100% of that of a standard cement mortar test block.
Description
Technical Field
The invention relates to the field of resource utilization of inorganic solid wastes, in particular to a method for preparing a volcanic ash active material from building muck containing quartz, mica and chlorite mineral phases.
Background
The Ningbo soft soil landform is mostly a coastal-phase silted plain, the soft soil coverage area is wide, and the construction engineering field is basically distributed on the soft soil layer. The main soft soil layer of Ningbo urban buildings has two layers: the first layer is composed of new sea-phase silted muddy soil, has large thickness and large water content, is mostly in a plastic state and has the thickness of 2-20 meters; the second layer is a Shangshuishi sea food layer with a thickness of 28-45 m, and has lower compressibility than the first layer and is in a soft plastic state. Ningbo soft soil has a sponge structure and a large-scale layer structure, and has poor water permeability due to the fact that the Ningbo soft soil contains more organic matters and clay minerals, has more clay grains, is rich in bound water, and has weak bonding force among particles. Because of the need to excavate the foundation, Ningbo construction sites have a large amount of mineral-containing, extremely fine clay waste, construction residue.
The clay is widely applied to preparing ceramics, cement, ceramsite and the like, but the waste clay of Ningbo construction sites is construction waste, has high water content, is not high in backfill curing strength as the clay, cannot be backfilled, is easy to cause environmental pollution and the like, so that the recycling of the construction waste clay is urgently needed to be solved.
Disclosure of Invention
The invention aims to provide a method for preparing a volcanic ash active material from construction slag containing quartz, mica and chlorite mineral phases.
The technical scheme for realizing the purpose of the invention is as follows: a method for preparing a pozzolanic active material from construction residues containing quartz, mica, chlorite mineral phases, comprising the steps of:
(1) drying the building residue soil containing quartz, mica and chlorite mineral phases to remove water;
(2) putting the mixture into a stirrer, spraying the activating auxiliary agent while stirring, stirring for 1-2 minutes, and uniformly mixing;
(3) and calcining the mixture at the calcining temperature of 400-825 ℃ for 1-4 hours, cooling to room temperature, and performing ball milling to obtain the pozzolan active mixed material.
Further, the components of the construction muck containing quartz, mica and chlorite mineral phases in percentage by mass are shown in the following table:
wherein the sum of the mass percentages of the components is 100%, and the ignition loss is 9-11%.
Further, the drying temperature is not higher than 105 ℃.
Furthermore, the activating auxiliary agent is an aqueous solution of sodium sulfate or sodium carbonate, the mass ratio of the construction residue soil to the aqueous solution of sodium sulfate or sodium carbonate is 100: 5-15, and the mass concentration of the aqueous solution of sodium sulfate or sodium carbonate is 10-20 wt%.
Furthermore, the temperature rise speed during calcination is controlled to be 5-10 ℃/min.
Furthermore, after ball milling, the residual content of 200-mesh sieve is controlled to be less than 5%.
Compared with the prior art, the invention has the remarkable advantages that:
(1) calcining the building residue soil containing mica and chlorite petrochemical phases at 400-825 ℃, preserving heat for 1-4 hours, and performing calcination activation treatment to ensure that the mica and chlorite mineral phases are amorphous and have good hydrolysis capacity and reaction capacity;
(2) the activated construction waste soil is subjected to activity inspection according to test materials and requirements for industrial waste residue activity of cement mixed materials specified in GB/T12957-2005 experimental method for industrial waste residue activity of cement mixed materials, and quantitative experiments of potential hydraulicity, pozzolanic activity and 28-day compressive strength ratio of cement. Test data show that the activated building muck has pozzolanic activity;
(3) the problem of resource recycling of waste building residue soil is effectively solved, the utilization rate is high, the problem of waste stacking is solved, and the benefit of additional products is increased.
Drawings
FIG. 1 is an XRD spectrum of the construction residue soil adopted by the invention.
FIG. 2 is a thermogravimetric-differential thermal analysis (TG-DSC) graph of the construction residue used in the present invention.
FIG. 3 is a schematic view of the thermal activation dissolution of the silica crystal structure in the construction residue adopted by the invention.
Detailed Description
The invention is explained in detail below with reference to the figures and examples.
The construction residue soil excavated in Ningbo building foundation pit construction, which is called Ningbo clay in the embodiment of the invention, has the water content of about 40 percent, and is subjected to component and mineral phase analysis, wherein the main mineral phases are mica, chlorite and quartz (see figure 1), and the chemical components of the construction residue soil (see table 1).
TABLE 1 Ningbo construction residual soil composition analysis
Loss on ignition data were tested separately. The composition analysis employed the results of the X-fluorescence analysis.
The principle of the invention is as follows:
(1) before calcination, the sodium sulfate solution and the sodium carbonate solution are mixed into clay, the activating assistant is uniformly distributed in the clay material by a spraying mode, and the two solutions are quickly absorbed by the clay because the clay particles are smaller than 100 mu m, have larger specific surface area and higher water absorption.
The mechanism of the damage of the sodium sulfate solution and the sodium carbonate to the quartz structure is as follows: the silicon dioxide in the quartz is connected with the top corners of other silicon-oxygen tetrahedrons by the four top corners of the silicon-oxygen tetrahedron, oxygen ions are shared, and the oxygen ions are called bridge oxygen to form silicon-oxygen network connection, so that the quartz structure is stable, and the volcanic ash activity is not existed at normal temperature. At high temperatures, sodium ions destroy the common oxygen ions. The heating reaction formula of sodium sulfate and sodium carbonate is as follows:
silica network oxygen on Na + Non-bridging oxygen, Na, present by cleavage of bridging oxygen under action + The ions are located near the cleaved bridging oxygen and are linked to the oxygen ions to form non-bridging oxygen ions. The silica network structure is broken and has an amorphous structure, the silica has volcanic ash activity, and the silica activation reaction process is as follows:
a schematic of the thermally activated dissolution of the silica crystal structure in a specific Ningbo clay is shown in FIG. 3.
(2) DSC analysis (activation temperature selection principle)
The thermal analysis (TG-DSC) curve of the building residue soil is shown in figure 2, and under the temperature of 400 ℃, dehydroxylation reaction does not occur, interlayer water and absorbed water are mainly removed, and the mineral crystal structure in the clay is basically not changed. At the temperature of 400-825 ℃, dehydroxylation reaction is mainly carried out to remove the structural water, and the mineral crystal structure is changed and is converted into an amorphous state. After 825 deg.c, there is a strong exothermic peak, which indicates that the mineral phase in clay above 825 deg.c produces phase change and is converted into other matter with stable crystal structure. Through the analysis, the mineral structure in the clay can be decomposed and converted into an amorphous state by selecting 400-825 ℃ as the calcination activation temperature, so that the volcanic ash has the volcanic ash activity.
(3) Through high-temperature calcination, hydroxyl in mineral crystal structures such as mica and chlorite in the clay escapes, the escape of the hydroxyl can cause the valence balance in the crystal structures to be damaged, the interatomic bonding strength is weakened, the crystal structures are changed into amorphous states, and the clay is changed into an activated state at the moment. The addition of sodium sulfate or sodium carbonate activating assistant during the calcination process promotes the disintegration and amorphization of quartz, mica and chlorite crystal structures in the clay, and realizes the further activation treatment of the building residue soil.
The method for activating the waste building residue soil comprises the following steps:
(1) putting the building residue soil into an oven to be dried for 24 hours at 105 ℃, and removing water;
(2) preparing anhydrous sodium sulfate or sodium carbonate into 10-20 wt% aqueous solution;
(3) and (3) putting the construction residue into a stirrer, then spraying sodium sulfate or sodium carbonate aqueous solution, stirring and spraying for 1-2 minutes to prepare a mixture, wherein the mass ratio of the construction residue to the sodium sulfate aqueous solution is 100: 5-15.
(4) And calcining the mixture, controlling the temperature rise speed to be 5-10 ℃/min, the calcining temperature to be 400-825 ℃, keeping the temperature for 1-4 hours, and then cooling to the room temperature.
(5) And (3) placing the calcined material into a ball mill for ball milling, and controlling the residual content of 200 meshes to be less than 5% to obtain the pozzolan active material.
(6) The activity test is carried out on the obtained pozzolan active material according to the test material and the requirement for the industrial waste residue activity of the cement mixed material specified in GB/T12957-2005 experimental method for the industrial waste residue activity of cement mixed materials, and the method for quantitative experiment of the potential hydraulicity, pozzolan activity and 28-day compressive strength ratio of cement. Test data show that the volcanic ash active material has volcanic ash activity, and the standard mortar strength retention rate of the volcanic ash active material doped with 30% is 98-102%.
Example 1: the preparation method of the volcanic ash active material comprises the following steps:
(1) placing Ningbo clay with components shown in Table 1 into an oven, drying at 105 deg.C for 24 hr, and removing water;
(2) preparing anhydrous sodium sulfate into a 20 wt% aqueous solution;
(3) putting Ningbo clay into a stirrer, then spraying a sodium sulfate aqueous solution, stirring and spraying for 1-2 minutes to prepare a mixture, wherein the mass ratio of Ningbo clay to the sodium sulfate aqueous solution is 100: 10.
(4) Calcining the mixture, controlling the heating rate at 10 ℃/min, the calcining temperature at 400 ℃, keeping the temperature for 4 hours, and then naturally cooling to room temperature.
(5) And (3) placing the calcined material into a ball mill for ball milling, and controlling the residual content of 200 meshes to be less than 5% to obtain the activated Ningbo clay, namely the volcanic ash active material.
According to the test material and the requirement for the industrial waste residue activity of the cement mixed material specified in GB/T12957-2005 Experimental method for the industrial waste residue activity of the cement mixed material, and the quantitative experiment method for the potential hydraulicity, the pozzolan activity and the 28-day compressive strength ratio of the cement, the Ningbo clay calcined and activated at 400 ℃ is subjected to activity test. The test data are shown in table 2 below.
TABLE 2
GB/T12957-2005 Experimental method for the activity of industrial waste residues of cement admixtures states that a test piece doped with 30% of a pozzolanic active substance is considered to have pozzolanic activity if the 28-day compressive strength of the test piece is greater than 65% of the compressive strength of a test piece not doped with a pozzolanic active substance. The test data shows that calcination of activated Ningbo clay at 400 ℃ has pozzolanic activity.
Example 2: the preparation method of the volcanic ash active material comprises the following steps:
(1) putting Ningbo clay into an oven, drying for 24h at 105 ℃, and removing water;
(2) preparing anhydrous sodium sulfate into a 20 wt% aqueous solution;
(3) putting Ningbo clay into a stirrer, then spraying a sodium sulfate aqueous solution, stirring and spraying for 1-2 minutes to prepare a mixture, wherein the mass ratio of Ningbo clay to the sodium sulfate aqueous solution is 100: 10.
(4) And calcining the mixture, controlling the heating rate at 10 ℃/min, the calcining temperature at 600 ℃, keeping the temperature for 2 hours, and then naturally cooling to room temperature.
(5) And (3) placing the calcined material into a ball mill for ball milling, and controlling the residual content of 200 meshes to be less than 5% to obtain the activated Ningbo clay, namely the volcanic ash active material.
According to the test material and the requirement for the industrial waste residue activity of the cement mixed material specified in GB/T12957-2005 Experimental method for the industrial waste residue activity of the cement mixed material, and the quantitative experiment method for the potential hydraulicity, the pozzolan activity and the 28-day compressive strength ratio of the cement, the Ningbo clay calcined and activated at the temperature of 600 ℃ is subjected to activity test. The test data are shown in table 3 below.
TABLE 3
GB/T12957-2005 Experimental method for the activity of industrial waste residues of cement admixtures states that a test piece doped with 30% of a pozzolanic active substance is considered to have pozzolanic activity if the 28-day compressive strength of the test piece is greater than 65% of the compressive strength of a test piece not doped with a pozzolanic active substance. The test data shows that calcination of activated Ningbo clay at 600 ℃ has pozzolanic activity.
Example 3: the preparation method of the volcanic ash active material comprises the following steps:
(1) putting Ningbo clay into an oven, drying for 24h at 105 ℃, and removing water;
(2) preparing anhydrous sodium sulfate into a 20 wt% aqueous solution;
(3) putting Ningbo clay into a stirrer, then spraying a sodium sulfate aqueous solution, stirring and spraying for 1-2 minutes to prepare a mixture, wherein the mass ratio of Ningbo clay to the sodium sulfate aqueous solution is 100: 5.
(4) Calcining the mixture, controlling the heating rate at 5 ℃/min, the calcining temperature at 800 ℃, keeping the temperature for 1 hour, and then naturally cooling to room temperature.
(5) And (3) placing the calcined material into a ball mill for ball milling, and controlling the residual content of 200 meshes to be less than 5% to obtain the activated Ningbo clay, namely the volcanic ash active material.
According to the test material and the requirement for the industrial waste residue activity of the cement mixed material specified in GB/T12957-2005 Experimental method for the industrial waste residue activity of the cement mixed material, and the quantitative experiment method for the potential hydraulicity, the pozzolan activity and the 28-day compressive strength ratio of the cement, the Ningbo clay calcined and activated at the temperature of 600 ℃ is subjected to activity test. The test data are shown in table 4 below.
TABLE 4
GB/T12957-2005 Experimental method for the activity of industrial waste residues of cement admixtures states that a test piece doped with 30% of a pozzolanic active substance is considered to have pozzolanic activity if the 28-day compressive strength of the test piece is greater than 65% of the compressive strength of a test piece not doped with a pozzolanic active substance. The test data shows that calcination of activated Ningbo clay at 800 ℃ has pozzolanic activity.
Example 4: the preparation method of the volcanic ash active material comprises the following steps:
(1) putting Ningbo clay into an oven, drying for 24h at 105 ℃, and removing water;
(2) preparing sodium carbonate into a 20 wt% aqueous solution;
(3) putting Ningbo clay into a stirrer, then spraying a sodium carbonate aqueous solution, stirring and spraying for 1-2 minutes to prepare a mixture, wherein the mass ratio of Ningbo clay to the sodium carbonate aqueous solution is 100: 10.
(4) Calcining the mixture, controlling the heating rate at 10 ℃/min, the calcining temperature at 800 ℃, keeping the temperature for 1 hour, and then naturally cooling to room temperature.
(5) And (3) placing the calcined material into a ball mill for ball milling, and controlling the residual content of 200 meshes to be less than 5% to obtain the activated Ningbo clay, namely the volcanic ash active material.
According to the test material and the requirement for the industrial waste residue activity of the cement mixed material specified in GB/T12957-2005 Experimental method for the industrial waste residue activity of the cement mixed material, and the quantitative experiment method for the potential hydraulicity, the pozzolan activity and the 28-day compressive strength ratio of the cement, the Ningbo clay calcined and activated at the temperature of 600 ℃ is subjected to activity test. The test data are shown in table 5 below.
TABLE 5
GB/T12957-2005 Experimental method for the activity of industrial waste residues of cement admixtures states that a test piece doped with 30% of a pozzolanic active substance is considered to have pozzolanic activity if the 28-day compressive strength of the test piece is greater than 65% of the compressive strength of a test piece not doped with a pozzolanic active substance. The test data shows that calcination of activated Ningbo clay at 600 ℃ has pozzolanic activity.
Claims (5)
1. A method for preparing a pozzolan active material from construction residues containing quartz, mica and chlorite mineral phases is characterized by comprising the following steps:
(1) drying the building residue soil containing quartz, mica and chlorite mineral phases to remove water;
(2) putting the mixture into a stirrer, spraying the activating auxiliary agent while stirring, stirring for 1-2 minutes, and uniformly mixing;
(3) calcining the mixture at 400-825 ℃ for 1-4 hours, then cooling to room temperature, and performing ball milling to obtain a pozzolan active mixed material;
wherein, the components of the building muck containing quartz, mica and chlorite mineral phases are shown in the following table in percentage by mass:
wherein the sum of the mass percentages of the components is 100%, and the ignition loss is 9-11%;
the activating auxiliary agent is an aqueous solution of sodium sulfate or sodium carbonate, and the mass concentration of the activating auxiliary agent is 10-20 wt%.
2. The method of claim 1, wherein the drying temperature is not greater than 105 ℃.
3. The method of claim 1, wherein the mass ratio of the construction residue soil to the activation aid is 100: 5 to 15.
4. The method according to claim 1, wherein the temperature rise rate during the calcination is controlled to 5 ℃/min to 10 ℃/min.
5. The method of claim 1, wherein the 200 mesh sieve is controlled to have less than 5% residue after ball milling.
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